HRID1879270
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of compound 112 and 4-bromo-3-methoxyaniline (1 eq.) in DCM (0.15 M) was added PPTS (1 eq.). The mixture was heated to reflux and stirred for one day. The mixture was cooled and the solids were removed by filtration and washed with dichloromethane. The filtrate was concentrated and purified by column chromatography (SiO2, PE:EtOAc with EtOAc from 1 to 15%) to give the title compound 113 (80%). 1H NMR (CDCl3) δ (ppm) 10.32 (br s, 1H), 7.32 (m, 5H), 7.20 (d, J 8.5, 1H), 6.19 (dd, J 8.5, 2.5, 1H), 6.11 (d, J 2.5, 1H), 5.03 (s, 1H), 4.21 (q, J 7.0, 2H), 3.50 (s, 3H), 1.32 (t, J 7.0, 3H).
WORKUP
后处理
- temperatureThe mixture was heated
- temperatureto reflux
- temperatureThe mixture was cooled
- customthe solids were removed by filtration
- washwashed with dichloromethane
- concentrationThe filtrate was concentrated
- custompurified by column chromatography (SiO2, PE:EtOAc with EtOAc from 1 to 15%)